反应详情

29.9 g (0.09 mol) of III-15 was dissolved in a mixed solution of 150 ml of toluene and 50 ml of pyridine, followed by addition of 9.42 g (0.12 mol) of acetyl chloride at 15°-20° C. over a period of 2 hours. The mixture was maintained at the same temperature for 2 hours and then at 40°-45° C. for another 2 hours. The reaction mixture was cooled below 10° C. and added with 300 ml of 3N hydrochloric acid. After separating the liquid phase, the organic layer was washed with water, 5% sodium hydrogencarbonate and water successively in that order and concentrated under reduced pressure. The residue was purified by column chromatography to give 33.0 g (98% yield) of benzyl 4'-(1-acetoxyethyl)-4-biphenylcarboxylate (IV-15).

1. temperatureThe mixture was maintained at the same temperature for 2 hours
2. temperatureThe reaction mixture was cooled below 10° C.
3. customAfter separating the liquid phase
4. washthe organic layer was washed with water, 5% sodium hydrogencarbonate and water successively in that order
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography